Dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry for the rapid and sensitive determination of UV filters in environmental water samples

• Published in: Analytical and bioanalytical chemistry Vol. 398; no. 2; pp. 995 - 1004
• Main Authors: Negreira, N, Rodríguez, I, Rubí, E, Cela, R
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Berlin/Heidelberg : Springer-Verlag 01.09.2010; Springer-Verlag; Springer
• Subjects: Acetone; Analytical Chemistry; Applied sciences; Biochemistry; Characterization and Evaluation of Materials; Chemical Fractionation - methods; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Dispersants; Dispersive liquid-liquid microextraction; Environmental Monitoring - economics; Environmental Monitoring - methods; Exact sciences and technology; Food Science; Gas chromatographic methods; Gas chromatography; Gas Chromatography-Mass Spectrometry - economics; Gas Chromatography-Mass Spectrometry - methods; GC-MS; Global environmental pollution; Laboratory Medicine; Liquid-liquid extraction; Monitoring/Environmental Analysis; Original Paper; Pollution; Rivers; Salicylates - analysis; Salicylates - isolation & purification; Sensitivity and Specificity; Spectrometric and optical methods; Spectrometry; Spectrum analysis; Standard deviation; Strategy; Strength; Sunscreening Agents - analysis; Sunscreening Agents - isolation & purification; Swimming Pools; Time Factors; UV filters; Water; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - isolation & purification; Water samples; GC-MS; UV filters; Dispersive liquid–liquid microextraction; Water samples; Water; Performance evaluation; Dispersive liquid―liquid microextraction; Microanalysis; Optimization; Sample preparation; Efficiency; Detection limit; pH; Standard deviation; Extraction; Solvent; Sample; Concentration; Method; Gas chromatography; Filter; Ionic strength; Volume; Linearity; Microextraction; Environment; Parameter; Strategy; Technique; Detection; Mass spectrometry; Acetone
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-010-4009-9

The performance of the dispersive liquid-liquid microextraction (DLLME) technique for the determination of eight UV filters and a structurally related personal care species, benzyl salicylate (BzS), in environmental water samples is evaluated. After extraction, analytes were determined by gas chromatography combined with mass spectrometry detection (GC-MS). Parameters potentially affecting the performance of the sample preparation method (sample pH, ionic strength, type and volume of dispersant and extractant solvents) were systematically investigated using both multi- and univariant optimization strategies. Under final working conditions, analytes were extracted from 10 mL water samples by addition of 1 mL of acetone (dispersant) containing 60 μL of chlorobenzene (extractant), without modifying either the pH or the ionic strength of the sample. Limits of quantification (LOQs) between 2 and 14 ng L⁻¹, inter-day variability (evaluated with relative standard deviations, RSDs) from 9% to 14% and good linearity up to concentrations of 10,000 ng L⁻¹ were obtained. Moreover, the efficiency of the extraction was scarcely affected by the type of water sample. With the only exception of 2-ethylhexyl-p-dimethylaminobenzoate (EHPABA), compounds were found in environmental water samples at concentrations between 6 ± 1 ng L⁻¹ and 26 ± 2 ng mL⁻¹. [graphic removed]